CN115961228A - Preparation method of titanium plate for deep drawing - Google Patents
Preparation method of titanium plate for deep drawing Download PDFInfo
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- CN115961228A CN115961228A CN202310014741.4A CN202310014741A CN115961228A CN 115961228 A CN115961228 A CN 115961228A CN 202310014741 A CN202310014741 A CN 202310014741A CN 115961228 A CN115961228 A CN 115961228A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000010936 titanium Substances 0.000 title claims abstract description 112
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 112
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000005096 rolling process Methods 0.000 claims abstract description 186
- 238000011282 treatment Methods 0.000 claims abstract description 149
- 238000000137 annealing Methods 0.000 claims abstract description 90
- 238000005098 hot rolling Methods 0.000 claims abstract description 72
- 238000000034 method Methods 0.000 claims abstract description 49
- 238000005097 cold rolling Methods 0.000 claims abstract description 40
- 238000005242 forging Methods 0.000 claims abstract description 34
- 238000003723 Smelting Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 3
- 239000000956 alloy Substances 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 77
- 238000005406 washing Methods 0.000 claims description 70
- 238000000227 grinding Methods 0.000 claims description 69
- 239000003513 alkali Substances 0.000 claims description 68
- 238000010438 heat treatment Methods 0.000 claims description 68
- 238000005554 pickling Methods 0.000 claims description 65
- 238000002791 soaking Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 229910003460 diamond Inorganic materials 0.000 claims description 16
- 239000010432 diamond Substances 0.000 claims description 16
- 239000011265 semifinished product Substances 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 230000010485 coping Effects 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000010008 shearing Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000004381 surface treatment Methods 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 16
- 239000013078 crystal Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 230000009286 beneficial effect Effects 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a preparation method of a titanium plate for deep drawing, which comprises the following steps: the method comprises the following steps: the Brinell hardness HB of the alloy is less than 95 and is 0 A The titanium sponge is used as a raw material, and a titanium ingot is obtained by twice smelting through a vacuum consumable arc smelting method; step two: forging a titanium ingot into a titanium plate blank in a one-way mode along the axial direction; step three: hot rolling and cogging, and rolling along the direction vertical to the forging direction to obtain a rough rolling blank; step four: hot rolling by a second fire, and rolling in the third rolling direction to obtain a second fire plate blank; step five: hot rolling with three heats, rolling along the direction vertical to the rolling direction of the step four to obtain a three-fire plate blank; step six: for three fire plate blanksPerforming surface treatment, annealing treatment and the like; step seven: cold rolling twice to obtain a cold-rolled sheet with the thickness of 0.4 +/-0.02 mm; step eight: and (5) annealing the finished product. The method efficiently manufactures the thin titanium plate for deep drawing with low cost and stable quality through the steps of unidirectional forging, reversing hot rolling, twice cold rolling, annealing without atmosphere protection or vacuum and the like.
Description
Technical Field
The invention belongs to the technical field of titanium alloy plates, and particularly relates to a preparation method of a titanium plate for deep drawing.
Background
Commercial pure titanium is prepared by smelting and casting sponge titanium into crystal ingots, and then processing the crystal ingots by plastic processing methods such as forging, rolling, extruding and the like. The mechanical property of the coarse columnar casting structure is poor, and the use of titanium is influenced, so that the titanium crystal ingot needs to be subjected to deformation such as forging, rolling and the like and annealing treatment, an ideal structure form is obtained, and the microstructure and the performance of the titanium plate are changed. However, the processing of commercial pure titanium has the difficulties of obvious anisotropy, easy hydrogen absorption at high temperature and the like, so that the preparation of the titanium often requires rigorous equipment and strict technical conditions.
At present, in order to uniformly refine original crystal grains, in the production of a thin titanium plate, a upsetting process is often required to be added in the forging process, the forging requirement is high, the forging time is long, and due to the fact that the temperature in the forging process is reduced quickly, multiple times of remelting and heating are caused, heat energy consumption is large, and the economical efficiency is poor. In addition, titanium is easy to react with oxygen and hydrogen in the air at high temperature to form a getter layer, which causes hydrogen embrittlement of the material and reduces the workability of the material, particularly, a thin plate is particularly serious, so that the annealing treatment furnace commonly used in the industry is an inert gas protection furnace or a vacuum furnace. However, the two annealing treatment furnaces have high manufacturing cost, high production cost and low production efficiency, and greatly limit the production capacity of the sheet. Moreover, the two annealing treatment furnaces can only adopt a roll type or stacking mode for charging, the temperature uniformity of the whole stack of materials is difficult to ensure, the performance difference of the same roll or the same sheet of plate is overlarge, and the use stability is influenced.
Patent application CN107723638A discloses a method for preparing a titanium plate for deep drawing, which uses sponge titanium with O content less than or equal to 0.05%, N content less than or equal to 0.006%, and Fe content less than or equal to 0.05% and not less than 0A grade as a raw material, carries out smelting casting and forging on the raw material, and carries out drawing and/or upsetting not less than two times in the forging process to prepare a slab with good structure and slight texture, and then the slab is subjected to hot rolling, cold rolling, reverse rolling, annealing and subsequent treatment to obtain a pure titanium plate with proper crystal grains, qualified performance and high cupping value. According to the method, time and energy are consumed in the forging link, the annealing of the finished plate needs more than 2 hours, and the cost is high and the efficiency is lower under the condition of vacuum and argon filling circulation. Patent application CN115323137A discloses a method for preparing a titanium plate for architectural decoration, which can increase the width and reduce the thickness of a titanium plate, improve the mechanical strength, control precision, roughness and flatness of the titanium plate product, and improve the color and roughness uniformity of surface roughening, but the annealing process is still performed under the protection of Ar atmosphere, which is too high in cost and not beneficial to popularization and application.
It is a urgent need in the titanium industry to simplify the production process of titanium materials and reduce the production cost. Particularly, in the traditional titanium plate production process, a new thought needs to be provided at key production nodes such as raw material selection, a smelting furnace, a forging mode, an annealing treatment mode, equipment, a rolling method and the like, and factors such as parameter design and/or control are supplemented, so that the simple preparation method of the deep-drawing thin titanium plate with stable quality and excellent comprehensive performance is obtained.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing a titanium plate for deep drawing, which adopts the steps of unidirectional forging, reverse hot rolling, twice cold rolling, annealing without atmosphere protection or vacuum and the like to efficiently manufacture a thin titanium plate for deep drawing with low cost and stable quality.
Specifically, the invention provides a preparation method of a titanium plate for deep drawing, which comprises the following steps:
the method comprises the following steps: the Brinell hardness HB of the alloy is less than 95 and is 0 A The titanium sponge is taken as a raw material, and a titanium ingot is obtained by twice smelting by a vacuum consumable arc smelting method;
step two: forging the titanium ingot in a one-way mode along the axial direction to obtain a titanium plate blank;
step three: hot rolling and cogging, heating the titanium plate blank to 800-850 ℃, and rolling along the direction vertical to the forging direction to obtain a rough rolling blank with the deformation rate of more than 85 percent; carrying out alkaline acid washing treatment and coping treatment on the rough rolling blank;
step four: hot rolling on second fire, heating the rough rolling blank to 750-800 ℃, rolling along the rolling direction in the third step, wherein the deformation rate is more than 65%, and performing fixed width shearing to obtain a second fire plate blank;
step five: hot rolling with three heats, heating the second hot plate blank to 750-800 ℃, rolling along the direction vertical to the rolling direction of the step four, and the deformation rate is more than 35%;
step six: sequentially carrying out a first round of alkali-acid washing treatment, polishing treatment, semi-finished product annealing treatment and a second round of alkali-acid washing treatment on the three fire plate blanks;
step seven: performing cold rolling twice along the rolling direction of the fifth step to obtain a cold-rolled sheet with the thickness of 0.4 +/-0.02 mm;
step eight: and carrying out finished product annealing treatment on the cold-rolled sheet.
The invention adopts 0 which is easily obtained from raw materials A The raw material of the titanium sponge is smelted into crystal ingots by a vacuum self-heating consumable arc smelting method (VAR), so that the difficulties and the cost of the raw material, equipment and process are low. And then, the titanium plate blank with the thickness H multiplied by the width B multiplied by the length L of (110-135 mm) multiplied by (600-700 mm) multiplied by (1000-1200 mm) is obtained by unidirectional forging, so that the efficiency and energy consumption losses such as overlong forging time and the like caused by the original upsetting process are avoided. In particular, the invention adopts a reversing hot rolling mode, namely, after the traditional unidirectional rolling, the slab is rotated by 90 degrees and then is unidirectionally rolled again. The method generates a large amount of (0001) basal plane textures in the rolling process, increases the deformation resistance of the hexagonal crystal grains in the height direction, improves the anisotropy of the plate, improves the plastic deformation ratio, produces the pure titanium plate in a TA1 rolling annealing state, and forms a large part of recrystallization textures from the inheritance of deformation texture orientation. The main slipping system of the plastic deformation of the titanium plate in the conventional full longitudinal rolling is
And &>
Pyramid surface<c+a>Slippage is generated to coordinate c-axis movement, the basal plane texture disappears, a pyramid texture is obtained, and finally anisotropy of the plate is generated. Eliminating the rolling texture is beneficial to improving the strength index and the plasticity index of the titanium plate. The subsequent two times of cold rolling can not only realize the further thinning of the titanium plate on the basis of improving the mechanical property of the titanium plate product, but also be beneficial to obtaining the required roughness and flatness. The subsequent annealing treatment of the single plate finished product is combined, so that the internal stress in rolling can be effectively released, and the stability of the size and the performance of the plate can be effectively improved. On the whole, the invention can prepare the thin pure titanium plate with the thickness of 0.4 +/-0.02 mm, which has fine and uniform crystal grains, weak anisotropy, high surface quality and stable size through the process links of raw material selection, efficient smelting, unidirectional forging, reversing hot rolling, twice cold rolling, surface treatment, annealing treatment and the like. And the corresponding heating furnace, hot rolling mill, cold rolling mill, annealing treatment equipment and the like adopted by the method are conventional equipment of a plate rolling mill, high-precision equipment such as an atmosphere protection furnace, a vacuum annealing furnace and the like is not needed, almost no additional investment is needed, the cost is low, and the popularization value is obvious.
Further, 0 A The titanium sponge comprises the following components in percentage by mass: less than or equal to 0.03 percent of iron, less than or equal to 0.05 percent of oxygen, less than or equal to 0.01 percent of nitrogen, less than or equal to 0.01 percent of carbon, less than or equal to 0.003 percent of hydrogen, less than or equal to 0.01 percent of silicon, less than or equal to 0.06 percent of chlorine, less than or equal to 0.01 percent of magnesium, less than or equal to 0.01 percent of manganese, less than or equal to 0.01 percent of nickel, less than or equal to 0.01 percent of chromium, less than or equal to 0.02 percent of the sum of other impurities, and the balance of titanium. The invention selects the 0A-grade sponge titanium, has low impurity percentage and ensures the deep tensile property of the finished product.
Furthermore, the thickness H, the width B and the length L of the titanium plate blank in the second step are (110-135 mm) × (600-700 mm) × (1000-1200 mm); and in the third step, heating the titanium plate blank to 800-850 ℃, preserving the heat for 120-150min, and rolling to obtain a rough rolling blank with the thickness of 12-15 mm. In the hot rolling cogging link, the deformation rate of the slab is high, the thickness of the slab is obviously reduced, and the adjustment of technical parameters such as the heating temperature, the heat preservation time and the like of the hot rolling cogging is an important condition for obtaining high-quality rough rolling slabs according to the size of the titanium slab.
And further, in the fourth step, heating the rough rolling blank to 750-800 ℃, preserving the heat for 15-20min, and rolling to obtain a double-fire plate blank with the thickness of 3-4 mm. Because the thickness of the rough rolling blank is obviously reduced relative to the thickness of the titanium plate blank, the heating and heat preservation time of the step four is correspondingly reduced relative to the step three, and the uniform heating of the plate blank can be ensured.
In the fourth step, the second hot rolling is carried out asynchronously by adopting an asynchronous rolling mill set, and the asynchronous rolling mill set is provided with at least 1 group of asynchronous rolling mills with different speeds and at least 1 group of asynchronous rolling mills with different diameters; the hot rolling direction is the same as the rolling direction of the step S3.3, and the pressure between the rollers of each rolling mill of the asynchronous rolling mill set is gradually increased along the rolling direction; upper roll speed V of asynchronous rolling mill 1 : lower roll speed V 2 1.3-1.5, the diameter R of the upper roll of the reducing asynchronous rolling mill 1 : diameter of lower roll R 2 Is 1: (1.1-1.3).
Further, in the fifth step, the second fire plate blank is reversed at 90 degrees, heated to 750-800 ℃, and subjected to unidirectional rolling after heat preservation for 10-15min to obtain a third fire plate blank with the thickness of 1.5-2 mm; in the sixth step, the semi-finished product annealing treatment comprises:
stacking 3-6 plate blanks;
heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 16-20min.
The reversing rolling can change the microscopic stress state of the material, so that the crystal grains are not twisted towards a certain fixed direction, the dislocation density of a deformation zone is high, the storage energy is high, sufficient driving force is provided for nucleation, the generation of fine crystal grains is promoted, the strength of a pyramid-shaped texture can be effectively reduced, and the anisotropy is improved. Compared with unidirectional rolling, the titanium plate blank rolled in a reversing way has the advantages that the structure is broken more fully, obvious anisotropy does not exist, the difference of mechanical properties of the plate in all directions is reduced, and the consistency of products is better.
The asynchronous rolling comprises asynchronous rolling at different speeds and asynchronous rolling at different diameters, and mainly utilizes the different linear speeds of an upper roller and a lower roller to enable a rolled piece to bear additional shear deformation. The asynchronous rolling mode fully utilizes the characteristics of severe plastic deformation, high precision and the like of asynchronous rolling, is beneficial to improving the quality and the dimensional precision of the plate blank, can relatively reduce the subsequent rolling passes, and improves the productivity.
The invention adopts a rolling mode combining reverse hot rolling and one-way asynchronous hot rolling, effectively weakens the rolling texture of the plate while efficiently reducing the thickness of the plate blank, is more beneficial to grain refinement and improves the comprehensive mechanical property. Due to the adoption of the specially designed hot rolling mode, the possible defect of uniform grain refinement of unidirectional forging is overcome integrally, and the product quality can be still ensured on the basis of improving the production efficiency by avoiding the redundant link of the original upsetting process.
In order to further improve the anisotropy of the plate and improve the deep drawing performance, the reversing thickness of the hot rolling three-fire process is required to be strictly executed according to a set cross ratio, so that the deformation degree before and after reversing tends to be balanced, and the longitudinal and transverse difference is reduced to the maximum extent. Preferably, the total deformation amount before hot rolling three-fire reversing is as follows: the total deformation after hot rolling three-fire reversing is 1-1.15, wherein the total deformation before hot rolling three-fire reversing is (the thickness of a titanium plate blank is H-the thickness of a two-fire plate blank is H) 1 ) H, the total deformation after hot rolling on three heats is (thickness H of the slab on two heats) 1 -finished product thickness H 2 )/H 1 . More preferably, the total deformation amount before hot rolling three-fire reversing is as follows: the total deformation after hot rolling three-fire reversing is 1-1.13.
Further, in the seventh step, cold rolling is carried out for one time to obtain a cold rolled blank with the thickness of 0.7-1.0 mm; then rolling to a cold-rolled sheet with the thickness of 0.4 +/-0.02 mm; performing intermediate annealing treatment and alkali-acid washing treatment between two times of cold rolling, wherein the intermediate annealing treatment comprises the following steps:
stacking 3-8 plate blanks;
heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 16-20min.
The intermediate annealing treatment and the two-time cold rolling process are combined, so that on one hand, the problem of poor plate shape is effectively improved by utilizing the high temperature and the proper tension condition of the annealing treatment relative to the cold rolling process, on the other hand, the internal stress of the one-time cold rolling is favorably released, and the damage of the plate blank caused by the two-time cold rolling is avoided. The intermediate annealing treatment is carried out by adopting a way of stacking and annealing the plate blanks, so that the advantages of the intermediate annealing treatment are exerted, and the treatment time is saved.
Further, in the eighth step, the single cold-rolled sheet is heated to 680 +/-10 ℃ on line by using an all-solid-state high-frequency induction heating device, and annealing treatment is carried out for 16-20min.
Preferably, an all-solid-state high-frequency induction heating device of 50-100kW can be used for online heating, the heating rate is 300-400 ℃/min, the temperature is heated to 680 +/-10 ℃, and an infrared thermometer is used for accurately measuring the temperature; after preserving heat for 3-5min, carrying out stepped cooling treatment, comprising the following steps:
s7.1: cooling to 400 ℃ at a speed of not higher than 40 ℃/min;
s7.2: cooling to 200 deg.C at a rate of 60 deg.C/min or less;
s7.3: cooling to room temperature at a rate of not higher than 80 deg.C/min.
And step eight, annealing the finished product, wherein although the continuous annealing conditions similar to the semi-finished product annealing treatment or the intermediate goods returning treatment can be adopted, the single-plate step annealing treatment is preferably adopted, so that the plate stays in a high-temperature section for a longer time, the internal stress is fully released, the micro and macro defects are reduced or avoided, and then the cooling speed is increased, thereby ensuring the goods returning quality and improving the treatment efficiency.
Further, the alkali acid washing treatment of the rough rolling blank, the three-hot plate blank and the cold rolling blank comprises the following steps:
A. alkali washing: soaking the plate blank in 460-520 ℃ alkali melt, and carrying out alkali washing for 5-15min; said alkali melt is composed of 85-95wt% NaOH and 5-15wt% NaNO 3 Forming;
B. primary acid washing: soaking the thin slab in a first acid solution at the temperature of below 60 ℃, pickling for less than 2min, and washing with water and drying; the first acid solution comprises: 5-15wt.% of 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the sheet bar in a second acid solution at a temperature below 60 ℃, and pickling for less than 5min; the second acid solution contains: 15-25wt% of HNO 3 1-2% wtHF and the balance water.
The titanium material is easy to form a gas suction layer at high temperature, the prior art is generally weakened by adopting protective atmosphere or vacuum environment, but the equipment requirement is high, and the cost is high. A large number of experiments show that the air suction layer can be well removed through alkali pickling treatment, and the effect is remarkable by removing the surface oxide skin through twice pickling and water explosion by soaking and alkali washing in molten alkali liquor. Preferably, in the sixth step, the treatment of the three-fire plate blank further comprises the step of adding a stripping treatment after the annealing treatment and the alkali pickling treatment of the semi-finished product, similar to the above secondary pickling, with the difference that the adopted HF concentration is 2-3wt%, the surface of the plate blank can be further uniformly corroded by about 10-20 μm, and the residual getter layer can be completely removed, and the whole processing process and the product performance are hardly influenced.
Further, the grinding treatment of the rough rolling blank and the three-fire plate blank adopts a diamond grinding wheel, and comprises the following steps:
s1, coarse grinding: the granularity of the rough grinding wheel is 100-150 meshes, the rotating speed is 1500-2000r/min, the feeding amount is 0.02 mm-0.05 mm each time, and the feeding speed of the diamond grinding wheel is 800 mm/min-1000 mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200-300 meshes, the rotating speed is 3500 r/min-4000 r/min, the feeding amount is less than 0.01mm each time, and the feeding speed is 300 mm/min-450 mm/min.
According to the requirements of the treatment process, the slab after the alkali-acid washing treatment is subjected to grinding wheel polishing so as to sufficiently remove the oxide skin on the surface and the surface defects appearing by rolling and the like. The slab after hot rolling and three heats is subjected to further treatment such as two times of cold rolling and the like, the three-fire slab is subjected to comprehensive surface treatment, annealing treatment and the like, the problem of an air suction layer formed in the early hot rolling high-temperature stage is solved in advance, the annealing treatment process with lower temperature and shorter time is adopted, the subsequent air suction layer is avoided or reduced, the influence of hydrogen embrittlement is relieved, the subsequent treatment pressure and difficulty can be effectively reduced, and the product quality is favorably improved.
By the method for preparing the titanium plate for deep drawing, the high-performance titanium plate with the thickness of 0.4 +/-0.02 mm, the yield strength of more than 180MPa, the tensile strength of more than 290MPa and the elongation after fracture of more than 65 percent can be prepared, the thickness of the high-performance titanium plate is less than the lower limit value of the plate thickness required by the national standard GB/T14845 (the titanium plate for a plate heat exchanger), and the mechanical property can reach and exceed the standard requirement, so that the use amount of the titanium material is saved, and the production cost is reduced.
The invention has the advantages that:
1) The invention adopts unidirectional forging and reversing hot rolling with specific cross ratio, and combines the reversing hot rolling with asynchronous hot rolling, thereby not only obviously saving forging time, but also effectively refining uniform original crystal grains, improving the anisotropy of the plate and comprehensively improving the mechanical property and the quality stability of the plate.
2) According to the invention, through alkali pickling and other treatments after three hot rolling and before cold rolling, the problem of an air suction layer formed in the early hot rolling high-temperature stage is solved in advance, and then an annealing treatment process with lower temperature and shorter time is adopted, so that the air suction layer generated by the subsequent annealing treatment is reduced, and the influence of hydrogen embrittlement is avoided; meanwhile, because the semi-finished product annealing treatment and the intermediate annealing treatment between two times of cold rolling both adopt slab stacking continuous annealing, each section of the slab is ensured to be in the same annealing treatment environment, the performance stability of the same sheet or even the same batch of plates is greatly improved, and the defects of long annealing time, poor temperature uniformity, high requirement on equipment and high cost of the traditional atmosphere gas protection or vacuum annealing furnace and other annealing processes are avoided.
3) The invention adopts the step annealing treatment of the finished veneer product, can effectively release the internal stress of the veneer in time by means of the conditions of high temperature and the like during the treatment, and avoids the damage of the subsequent treatment to the veneer or the unexpected change of the size of the veneer; and the annealing mode is favorable for slowly and fully releasing the internal stress of the plate at the high-temperature section, and then the temperature is accelerated to improve the treatment efficiency, thereby taking the efficiency and the product quality into consideration.
Drawings
The above and other objects, features and advantages of exemplary embodiments of the present disclosure will become readily apparent from the following detailed description, which proceeds with reference to the accompanying drawings. In the drawings, several embodiments of the invention are shown by way of example and not by way of limitation, wherein the dimensions, deformation ratios, etc. of the slab treatment process are shown by way of example only.
FIG. 1 is a schematic flow chart of the production process of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to fig. 1 and the embodiments.
A preparation method of a titanium plate for deep drawing comprises the following steps:
the method comprises the following steps: the Brinell hardness HB of 0 below 95 is adopted A The titanium sponge is taken as a raw material, and a titanium ingot is obtained by twice smelting by a vacuum consumable arc smelting method; 0 A The titanium sponge comprises the following components in percentage by mass: less than or equal to 0.03 percent of iron, less than or equal to 0.05 percent of oxygen, less than or equal to 0.01 percent of nitrogen, less than or equal to 0.01 percent of carbon, less than or equal to 0.003 percent of hydrogen, less than or equal to 0.01 percent of silicon, less than or equal to 0.06 percent of chlorine, less than or equal to 0.01 percent of magnesium, less than or equal to 0.01 percent of manganese, less than or equal to 0.01 percent of nickel, less than or equal to 0.01 percent of chromium, less than or equal to 0.02 percent of the sum of other impurity contents, and the balance of titanium;
step two: forging a titanium ingot into a titanium plate blank in a one-way mode along the axial direction, wherein the thickness H, the width B and the length L of the titanium plate blank are (110-135 mm) × (600-700 mm) × (1000-1200 mm);
step three: hot rolling and cogging, heating the titanium plate blank to 800-850 ℃, keeping the temperature for 120-150min, and then rolling along the direction vertical to the forging direction to obtain a rough rolling blank with the deformation rate of more than 85 percent to obtain a rough rolling blank with the thickness of 12-15 mm;
and carrying out alkali pickling treatment and coping treatment on the rough rolling blank.
Step four: hot rolling on second fire, heating the rough rolling blank to 750-800 ℃, preserving heat for 15-20min, rolling along the rolling direction of the third step, wherein the deformation rate is more than 65%, and shearing at constant width to obtain a second fire plate blank with the thickness of 3-4 mm; the rolling is carried out by asynchronous hot rolling by adopting an asynchronous rolling mill set, and the asynchronous rolling mill set is provided with at least 1 group of asynchronous rolling mills with different speeds and at least 1 group of asynchronous rolling mills with different diameters; the hot rolling direction is the same as the rolling direction of the step S3.3, the pressure between the rollers of each rolling mill of the asynchronous rolling mill set is gradually increased along the rolling direction, and the upper roller speed V1 of the asynchronous rolling mill at different speeds is as follows: the lower roll speed V2 is 1.3-1.5, the diameter R1 of the upper roll of the reducing asynchronous rolling mill is as follows: lower roll diameter R2 is 1: (1.1-1.3);
step five: hot rolling with three heats, heating the second hot plate blank to 750-800 ℃, preserving heat for 10-15min, rolling along the direction vertical to the rolling direction of the fourth step, wherein the deformation rate is more than 35%, and obtaining the third hot plate blank with the thickness of 1.5-2 mm;
step six: sequentially carrying out alkali pickling treatment, polishing treatment, semi-finished product annealing treatment and alkali pickling treatment on the three fire plate blanks; preferably, after the semi-finished product is annealed and subjected to acid reduction and pickling, a channel removing treatment is further arranged; the annealing treatment comprises the following steps:
stacking 3-6 plate blanks;
heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 16-20min.
Step seven: performing cold rolling twice along the rolling direction of the fifth step, performing cold rolling once to obtain a cold rolling blank with the thickness of 0.7-1.0mm, and then performing cold rolling to obtain a cold rolling plate with the thickness of 0.4 +/-0.02 mm; performing intermediate annealing treatment and alkali acid washing treatment between two times of cold rolling, wherein the intermediate annealing treatment comprises the following steps:
stacking 3-8 plate blanks;
heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 16-20min.
Step eight: and carrying out finished product annealing treatment on the cold-rolled sheet. And (3) heating the single cold-rolled sheet to 680 +/-10 ℃ on line by using an all-solid-state high-frequency induction heating device, and annealing for 16-20min.
Specifically, an all-solid-state high-frequency induction heating device of 50-100kW is used for carrying out online heating, the heating rate is 300-400 ℃/min, the heating is carried out to 680 +/-10 ℃, and the temperature is accurately measured by an infrared thermometer; after preserving heat for 3-5min, carrying out step cooling treatment, comprising the following steps:
s7.1: cooling to 400 ℃ at a speed of not higher than 40 ℃/min;
s7.2: cooling to 200 deg.C at a rate of 60 deg.C/min or less;
s7.3: cooling to room temperature at a rate of not higher than 80 deg.C/min.
The alkali pickling treatment of the rough rolling blank, the three-fire plate blank and the cold rolling blank comprises the following steps:
A. alkali washing: soaking the plate blank in alkali melt liquid at 460-520 ℃ and carrying out alkali washing for 5-15min; the alkali molten liquid is 85-95wt% NaOH and 5-15wt% NaNO 3 Composition is carried out;
B. primary acid washing: soaking the thin slab in a first acid solution at the temperature of below 60 ℃, pickling for less than 2min, and washing with water and drying; the first acid solution contains: 5-15wt.% of 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the sheet billet in a second acid solution at the temperature of below 60 ℃, and pickling for less than 5min; the second acid solution contains: 15-25wt% of HNO 3 1-2% wtHF and the balance water.
Wherein, the time of alkali washing, primary acid washing and secondary acid washing can be relatively reduced along with the reduction of the thickness of the plate.
The grinding treatment of the rough rolling blank and the three-fire plate blank adopts a diamond grinding wheel, and comprises the following steps:
s1, coarse grinding: the granularity of the rough grinding wheel is 100-150 meshes, the rotating speed is 1500-2000r/min, the feeding amount is 0.02 mm-0.05 mm each time, and the feeding speed of the diamond grinding wheel is 800 mm/min-1000 mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200-300 meshes, the rotating speed is 3500 r/min-4000 r/min, the feeding amount is less than 0.01mm each time, and the feeding speed is 300 mm/min-450 mm/min.
Example 1
A preparation method of a titanium plate for deep drawing comprises the following steps:
the method comprises the following steps: using a Brinell hardness HB of 90 of 0 A Titanium sponge grade is used as raw material, titanium ingot is obtained by twice smelting by using vacuum consumable arc smelting method, 0 A The titanium sponge comprises the following components in percentage by mass: 0.023 percent of iron, 0.035 percent of oxygen, 0.002 percent of nitrogen, 0.007 percent of carbon, 0.001 percent of hydrogen, 0.002 percent of silicon, 0.003 percent of chlorine, 0.003 percent of magnesium, 0.002 percent of manganese, 0.001 percent of nickel, 0.002 percent of chromium, 0.015 percent of the total content of other impurities and the balance of titanium.
Step two: forging a titanium ingot into a titanium plate blank along the axial direction in a one-way mode, wherein the thickness H, the width B, the length L of the titanium plate blank are 130mm, 650mm and 1100mm;
step three: and (3) hot rolling and cogging, heating the titanium plate blank to 820 ℃, preserving heat for 135min, and then rolling along the direction vertical to the forging direction to obtain a rough rolling blank with the thickness of 12 mm.
Carrying out alkali-acid washing treatment and coping on a rough rolling blank with the thickness of 12mm, wherein the alkali-acid washing treatment comprises the following steps:
A. alkali washing: soaking the plate blank in 500 ℃ alkali molten liquid, and carrying out alkali washing for 10min; the alkali melt was converted from 90wt% to NaOH and 10wt% to NaNO 3 Composition is carried out;
B. primary acid washing: soaking the thin slab in a first acid solution at 55 ℃, pickling for 1.5min, and washing with water and drying; the first acid solution contains: 10wt% of H 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the thin slab in a second acid solution at the temperature of below 60 ℃, and pickling for 4.5min; the second acid solution contains: 20wt% of HNO 3 1.5% wthf and the balance water.
Carrying out grinding wheel coping treatment on the plate blank subjected to the alkali and acid washing treatment by adopting a diamond grinding wheel, and comprising the following steps of:
s1, coarse grinding: the granularity of the grinding wheel is roughly ground to 100 meshes, the rotating speed is 1800r/min, the feeding amount is 0.03mm each time, and the feeding speed of the diamond grinding wheel is 900mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200 meshes, the rotating speed is 3800r/min, the feeding amount is 0.005mm each time, and the feeding speed is 400mm/min.
Step four: hot rolling on second fire, heating the rough rolling blank to 780 ℃, preserving heat for 20min, rolling along the rolling direction in the third step, and shearing at constant width to obtain a second fire plate blank with the thickness of 3.5 mm; the rolling is carried out by asynchronous hot rolling by adopting an asynchronous rolling mill set, and the asynchronous rolling mill set is provided with at least 1 group of asynchronous rolling mills with different speeds and at least 1 group of asynchronous rolling mills with different diameters; and the pressure between the rollers of each rolling mill of the asynchronous rolling mill set is gradually increased along the rolling direction, and the upper roller speed V1 of the asynchronous rolling mill at different speeds is as follows: the lower roll speed V2 is 1.4, the diameter R1 of the upper roll of the reducing asynchronous rolling mill is as follows: lower roll diameter R2 is 1:1.2;
step five: and (3) hot rolling with three heats, namely heating the second-fire plate blank to 780 ℃, preserving the heat for 15min, and rolling in the direction perpendicular to the rolling direction in the fourth step to obtain a third-fire plate blank with the thickness of 2 mm.
Step six: sequentially carrying out first round of alkali pickling, polishing, semi-finished product annealing treatment and second round of alkali pickling on three fire plate blanks with the thickness of 2 mm:
the steps of the first round of alkali pickling and the second round of alkali pickling are the same as the steps of the alkali pickling treatment of the previous rough rolled blank, and the difference is that the alkali pickling time is 8min, the primary pickling time is 1min, and the secondary pickling time is 3min;
the grinding wheel grinding treatment is the same as the grinding wheel grinding treatment of the previous rough rolling blank;
annealing treatment of a semi-finished product:
stacking the 4 plate blanks;
and heating the stacked plate blanks to 680 +/-10 ℃ by using an electric furnace, and annealing for 18min.
Step seven: and (5) carrying out cold rolling twice along the rolling direction of the step five:
carrying out primary cold rolling to obtain a cold-rolled blank with the thickness of 0.8 mm;
intermediate annealing treatment: stacking the 6 plate blanks; heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 17min;
the alkaline pickling treatment has the same steps as the alkaline pickling treatment of the rough rolled blank, and is characterized in that the alkaline pickling time is 5min, the primary pickling time is 0.5min, and the secondary pickling time is 1.5min;
and then rolled to a cold-rolled sheet with a thickness of 0.39 mm.
Step eight: and carrying out finished product annealing treatment on the cold-rolled sheet. And (3) carrying out on-line heating on the single cold-rolled sheet by using a 75kW all-solid-state high-frequency induction heating device, wherein the heating rate is 350 ℃/min, the heating is carried out to 680 +/-10 ℃, and an infrared thermometer is used for accurately measuring the temperature. After the heat preservation time is 5min, carrying out step cooling treatment for about 13.5min, and comprising the following steps:
s7.1: cooling to 400 ℃ at the speed of 40 ℃/min;
s7.2: cooling to 200 deg.C at a rate of 50 deg.C/min;
s7.3: and cooling to room temperature at the speed of 75 ℃/min to obtain a finished titanium plate with the thickness of 0.39 mm.
Example 2
A preparation method of a titanium plate for deep drawing comprises the following steps:
the method comprises the following steps: using a Brinell hardness HB of 88 of 0 A The titanium sponge is produced with titanium sponge as material and through twice vacuum consumable arc smelting processSmelting to obtain titanium ingot, 0 A The titanium sponge comprises the following components in percentage by mass: 0.018% of iron, 0.032% of oxygen, 0.004% of nitrogen, 0.008% of carbon, 0.001% of hydrogen, 0.001% of silicon, 0.004% of chlorine, 0.002% of magnesium, 0.002% of manganese, 0.003% of nickel, 0.004% of chromium, 0.013% of the total content of other impurities and the balance of titanium.
Step two: forging a titanium ingot into a titanium plate blank in a one-way mode along the axial direction, wherein the thickness H, the width B, the length L of the titanium plate blank are 125mm, 640mm and 1120mm;
step three: and (3) hot rolling and cogging, heating the titanium plate blank to 820 ℃, preserving heat for 125min, and then rolling along the direction vertical to the forging direction to obtain a rough rolling blank with the thickness of 11 mm.
Carrying out alkaline and acid washing treatment and coping on a rough rolling blank with the thickness of 11mm, wherein the alkaline and acid washing treatment comprises the following steps:
A. alkali washing: soaking the plate blank in 500 ℃ alkali molten liquid, and carrying out alkali washing for 9min; the alkali melt was converted from 90wt% to NaOH and 10wt% to NaNO 3 Composition is carried out;
B. primary acid washing: soaking the thin slab in a first acid solution at 55 ℃, pickling for 1.5min, and washing with water and drying; the first acid solution contains: 10wt% of H 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the thin slab in a second acid solution at the temperature of below 60 ℃, and pickling for 4min; the second acid solution contains: 20wt% of HNO 3 1.5% wtHF and balance water.
Carrying out grinding wheel coping treatment on the plate blank subjected to the alkali and acid washing treatment by adopting a diamond grinding wheel, and comprising the following steps of:
s1, coarse grinding: the granularity of the grinding wheel is roughly ground to 100 meshes, the rotating speed is 1800r/min, the feeding amount is 0.03mm each time, and the feeding speed of the diamond grinding wheel is 900mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200 meshes, the rotating speed is 3800r/min, the feeding amount is 0.005mm each time, and the feeding speed is 400mm/min.
Step four: hot rolling on second fire, heating the rough rolling blank to 780 ℃, preserving heat for 20min, rolling along the rolling direction in the third step, and shearing at constant width to obtain a second fire plate blank with the thickness of 3.6 mm; the rolling is carried out by asynchronous hot rolling by adopting an asynchronous rolling mill set, and the asynchronous rolling mill set is provided with at least 1 group of asynchronous rolling mills with different speeds and at least 1 group of asynchronous rolling mills with different diameters; the hot rolling direction is the same as the rolling direction of the step S3.3, the pressure between the rollers of each rolling mill of the asynchronous rolling mill set is gradually increased along the rolling direction, and the upper roller speed V1 of the asynchronous rolling mill at different speeds is as follows: the lower roll speed V2 is 1.4, the diameter R1 of the upper roll of the reducing asynchronous rolling mill is as follows: lower roll diameter R2 is 1:1.2;
step five: and (4) hot rolling with three heats, heating the second hot plate blank to 780 ℃, preserving the heat for 15min, and rolling in the direction perpendicular to the rolling direction in the fourth step to obtain a third hot plate blank with the thickness of 2.1 mm.
Step six: sequentially carrying out a first round of alkali pickling, polishing, semi-finished product annealing treatment and a second round of alkali pickling on three fire plate blanks with the thickness of 2.1 mm:
the steps of the first round of alkali pickling and the second round of alkali pickling are the same as the steps of the alkali pickling treatment of the rough rolling blank in the previous time, and the difference is that the alkali pickling time is 7min, the primary pickling time is 1min, and the secondary pickling time is 3min;
the grinding wheel grinding treatment is the same as the grinding wheel grinding treatment of the previous rough rolling blank;
annealing treatment of a semi-finished product:
stacking the 4 plate blanks;
and heating the stacked plate blanks to 680 +/-10 ℃ by using an electric furnace, and annealing for 18min.
Step seven: and (5) carrying out cold rolling twice along the rolling direction of the step five:
carrying out primary cold rolling to obtain a cold-rolled blank with the thickness of 0.8 mm;
intermediate annealing treatment: stacking the 6 plate blanks; heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 17min;
the alkaline pickling treatment has the same steps as the alkaline pickling treatment of the rough rolled blank, and is characterized in that the alkaline pickling time is 5min, the primary pickling time is 0.5min, and the secondary pickling time is 1.5min;
and then rolled to a cold-rolled sheet with a thickness of 0.40 mm.
Step eight: annealing the cold-rolled sheet, and heating the single cold-rolled sheet on line by using a 75kW all-solid-state high-frequency induction heating device at a heating rate of 350 ℃/min to 680 +/-10 ℃ and accurately measuring the temperature by using an infrared thermometer; after the heat preservation time is 4.5min, carrying out step cooling treatment for about 14min, and comprising the following steps:
s7.1: cooling to 400 ℃ at the speed of 40 ℃/min;
s7.2: cooling to 200 deg.C at a rate of 50 deg.C/min;
s7.3: and cooling to room temperature at the speed of 60 ℃/min to obtain a finished titanium plate with the thickness of 0.40 mm.
Example 3
A preparation method of a titanium plate for deep drawing comprises the following steps:
the method comprises the following steps: using a Brinell hardness HB of 92 of 0 A Titanium sponge grade is used as raw material, titanium ingot is obtained by twice smelting by using vacuum consumable arc smelting method, 0 A The titanium sponge comprises the following components in percentage by mass: 0.027% of iron, 0.045% of oxygen, 0.003% of nitrogen, 0.005% of carbon, 0.001% of hydrogen, 0.002% of silicon, 0.005% of chlorine, 0.001% of magnesium, 0.002% of manganese, 0.003% of nickel, 0.002% of chromium, 0.016% of the total content of other impurities and the balance of titanium.
Step two: forging a titanium ingot into a titanium plate blank in a one-way mode along the axial direction, wherein the thickness H, the width B, the length L and the length of the titanium plate blank are 128mm, 620mm and 1080mm;
step three: and (3) hot rolling cogging, namely heating the titanium plate blank to 820 ℃, preserving heat for 130min, and then rolling along the direction vertical to the forging direction to obtain a rough rolling blank with the thickness of 11.5 mm.
Carrying out alkaline and acid washing treatment and coping on a rough rolling blank with the thickness of 11.5mm, wherein the alkaline and acid washing treatment comprises the following steps:
A. alkali washing: soaking the plate blank in 500 ℃ alkali molten liquid, and carrying out alkali washing for 10min; alkali melt by 90wt% NaOH and 10wt% NaNO 3 Forming;
B. primary acid washing: soaking the thin slab in a first acid solution at 55 ℃, pickling for 1.5min, and washing with water and drying; the first acid solution contains: 10wt% of H 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the sheet billet in a second acid solution at the temperature of below 60 ℃ and pickling for 4min; the second acid solution contains: 20wt% of HNO 3 1.5% wtHF and balance water.
Carrying out grinding wheel coping treatment on the plate blank subjected to the alkali and acid washing treatment by adopting a diamond grinding wheel, and comprising the following steps of:
s1, coarse grinding: the granularity of the grinding wheel is roughly ground to be 100 meshes, the rotating speed is 1800r/min, the feeding amount is 0.03mm each time, and the feeding speed of the diamond grinding wheel is 900mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200 meshes, the rotating speed is 3800r/min, the feeding amount is 0.005mm each time, and the feeding speed is 400mm/min.
Step four: hot rolling on second fire, heating the rough rolling blank to 780 ℃, preserving heat for 20min, rolling along the rolling direction in the third step, and shearing at constant width to obtain a second fire plate blank with the thickness of 3.3 mm; the rolling is carried out by asynchronous hot rolling by adopting an asynchronous rolling mill set, and the asynchronous rolling mill set is provided with at least 1 group of asynchronous rolling mills with different speeds and at least 1 group of asynchronous rolling mills with different diameters; the hot rolling direction is the same as the rolling direction of the step S3.3, the pressure between the rollers of each rolling mill of the asynchronous rolling mill set is gradually increased along the rolling direction, and the upper roller speed V1 of the asynchronous rolling mill at different speeds is as follows: the lower roll speed V2 is 1.4, the diameter R1 of the upper roll of the reducing asynchronous rolling mill is as follows: lower roll diameter R2 is 1:1.2;
step five: and (4) hot rolling with three heats, heating the second hot plate blank to 780 ℃, preserving the heat for 15min, and rolling in the direction perpendicular to the rolling direction in the fourth step to obtain the third hot plate blank with the thickness of 1.9 mm.
Step six: sequentially carrying out a first round of alkali pickling, polishing, annealing treatment and a second round of alkali pickling on three fire plate blanks with the thickness of 1.9 mm:
the steps of the first round of alkali pickling and the second round of alkali pickling are the same as the steps of the alkali pickling treatment of the previous rough rolling blank, and the difference is that the alkali pickling time is 8min, the primary pickling time is 1min, and the secondary pickling time is 3min;
the grinding wheel grinding treatment is the same as the grinding wheel grinding treatment of the previous rough rolling blank;
annealing treatment of a semi-finished product:
stacking the 4 plate blanks;
and heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and annealing for 18min.
Step seven: and (5) carrying out cold rolling twice along the rolling direction of the step five:
carrying out primary cold rolling to obtain a cold-rolled blank with the thickness of 0.8 mm;
intermediate annealing treatment: stacking the 6 plate blanks; heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 17min;
the alkaline pickling treatment has the same steps as the alkaline pickling treatment of the rough rolled blank, and is characterized in that the alkaline pickling time is 5min, the primary pickling time is 0.5min, and the secondary pickling time is 1.5min;
and then rolled to a cold-rolled sheet with a thickness of 0.41 mm.
Step eight: and carrying out finished product annealing treatment on the cold-rolled sheet. Carrying out on-line heating on a single cold-rolled sheet by using a 75kW all-solid-state high-frequency induction heating device, wherein the heating rate is 350 ℃/min, the heating is carried out to 680 +/-10 ℃, and an infrared thermometer is used for accurately measuring the temperature; after the heat preservation time is 4min, carrying out step cooling treatment for about 15, comprising the following steps:
s7.1: cooling to 400 ℃ at the speed of 35 ℃/min;
s7.2: cooling to 200 deg.C at a rate of 50 deg.C/min;
s7.3: and cooling to room temperature at the speed of 60 ℃/min to obtain a finished titanium plate with the thickness of 0.41 mm.
Comparative example 1
The comparative example uses the same steps one to two, six to eight and surface treatment as example 1, and the difference is mainly that the steps three to five use unidirectional hot rolling, specifically:
step three: hot rolling and cogging, namely heating a titanium plate blank with the thickness H multiplied by the width B multiplied by the length L of 130mm multiplied by 650mm multiplied by 1100mm to 820 ℃, and preserving heat for 135min; rolling along the forging direction (namely the length direction of the titanium plate blank) to obtain a rough rolling blank with the thickness of 12 mm;
carrying out alkaline and acid washing treatment and coping on a rough rolling blank with the thickness of 12mm, wherein the alkaline and acid washing treatment comprises the following steps:
A. alkali washing: soaking the plate blank in 500 ℃ alkali molten liquid, and carrying out alkali washing for 10min; the alkali melt was converted from 90wt% to NaOH and 10wt% to NaNO 3 Forming;
B. primary acid washing: soaking the thin slab in a first acid solution at 55 ℃, pickling for 1.5min, and washing with water and drying; the first acid solution contains: 10wt% of H 2 SO 4 And the balance being water；
C. Secondary acid washing: soaking the sheet billet in a second acid solution at the temperature of below 60 ℃ and pickling for 4.5min; the second acid solution contains: 20wt% of HNO 3 1.5% wtHF and balance water.
Carrying out grinding wheel coping treatment on the plate blank subjected to the alkali and acid washing treatment by adopting a diamond grinding wheel, and comprising the following steps of:
s1, coarse grinding: the granularity of the grinding wheel is roughly ground to be 100 meshes, the rotating speed is 1800r/min, the feeding amount is 0.03mm each time, and the feeding speed of the diamond grinding wheel is 900mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200 meshes, the rotating speed is 3800r/min, the feeding amount is 0.005mm each time, and the feeding speed is 400mm/min.
Step four: hot rolling on second fire, heating the rough rolling blank to 780 ℃, preserving heat for 20min, rolling along the rolling direction in the third step, and shearing at constant width to obtain a second fire plate blank with the thickness of 3.5 mm;
step five: hot rolling with three heats, heating the second hot plate blank to 780 ℃, and keeping the temperature for 15min; and rolling along the rolling direction of the step four to obtain a three-fire plate blank with the thickness of 2 mm.
And then sequentially carrying out the six steps to the eight steps to obtain a titanium plate sample with the thickness of 0.39 mm.
Comparative example 2
This comparative example uses the same steps one, two and six as example 1, with the main difference being that steps three to five use single direction hot rolling, step seven uses two times of cold rolling without intermediate annealing, and step eight uses ordinary annealing. The second step sequentially comprises the following steps:
step three: hot rolling and cogging, heating a titanium plate blank with the thickness H multiplied by the width B multiplied by the length L of 130mm multiplied by 650mm multiplied by 1100mm to 820 ℃, and preserving heat for 135min; rolling in the forging direction (i.e. the length direction of the titanium plate blank) to obtain a rough rolled blank with the thickness of 12 mm.
Carrying out alkaline and acid washing treatment and coping on a rough rolling blank with the thickness of 12mm, wherein the alkaline and acid washing treatment comprises the following steps:
A. alkali washing: soaking the plate blank in 500 ℃ alkali molten liquid, and carrying out alkali washing for 10min; the alkali melt was converted from 90wt% to NaOH and 10wt% to NaNO 3 Composition is carried out;
B. at a timeAcid washing: soaking the sheet billet in a first acid solution at 55 ℃, pickling for 1.5min, and washing with water for drying; the first acid solution contains: 10wt% of H 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the sheet billet in a second acid solution at the temperature of below 60 ℃ and pickling for 4.5min; the second acid solution contains: 20wt% of HNO 3 1.5% wtHF and balance water.
Carrying out grinding wheel coping treatment on the plate blank subjected to the alkali and acid washing treatment by adopting a diamond grinding wheel, and comprising the following steps of:
s1, coarse grinding: the granularity of the grinding wheel is roughly ground to be 100 meshes, the rotating speed is 1800r/min, the feeding amount is 0.03mm each time, and the feeding speed of the diamond grinding wheel is 900mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200 meshes, the rotating speed is 3800r/min, the feeding amount is 0.005mm each time, and the feeding speed is 400mm/min.
Step four: hot rolling on second fire, heating the rough rolling blank to 780 ℃, preserving heat for 20min, rolling along the same direction of the third step, and shearing at constant width to obtain a second fire plate blank with the thickness of 3.5 mm;
step five: hot rolling with three heats, heating the second hot plate blank to 780 ℃, and preserving heat for 15min; and rolling in the same direction in the four steps to obtain the three-fire plate blank with the thickness of 2 mm.
The same procedure six as in example 1 was used;
step seven: and (5) cold rolling twice, wherein the rolling directions are the same as those of the step five, and the cold rolling method comprises the following steps: carrying out primary cold rolling to obtain a cold-rolled blank with the thickness of 0.8 mm; and then rolled to a cold-rolled sheet with a thickness of 0.39 mm.
Step eight: and heating the single cold-rolled sheet to 680 +/-10 ℃ by using an electric furnace, and annealing for 18min to obtain a titanium sheet sample with the thickness of 0.39 mm.
Comparative example 3
The titanium plate sample for the plate heat exchanger of the national standard GB/T14845 is adopted in the comparative example.
The room temperature mechanical properties of examples 1 to 3 and comparative examples 1 to 2 were tested. Specific results are shown in table 1:
TABLE 1 comparison of the Performance of examples 1-3 and comparative examples 1-3
The thickness measurement was performed by taking 6 measurement points for the samples of example 1 and comparative examples 1 to 2, and the same plate difference (unit: mm) was calculated, and the specific numbers are shown in Table 2:
table 2 thickness test results of example 1 and comparative examples 1 to 2
The performance of the finished titanium plate produced by the embodiment 1-3 of the invention reaches and exceeds the national standard. It is worth pointing out that the TA1 plate produced by the preparation method of the invention has the thickness less than the lower limit of the plate thickness required by GB/T14845, but has better mechanical property, is beneficial to saving the use amount of titanium materials and reducing the production cost. In contrast, comparative examples 1 and 2 can basically meet the requirement of GB/T14845, but have no obvious performance advantages, and have obviously less comprehensive performance such as mechanics and the like compared with examples 1-3, which is mainly due to the difference of selection and combination of the preparation processes between reversing hot rolling and unidirectional rolling, so that the differences of the uniformity, the anisotropy and the like of the plate crystal grains are caused. In addition, timely annealing treatment is beneficial to the release of the internal stress of the plate, the rolling effect is improved, and the comprehensive properties of the final plate, such as mechanical property, dimensional stability, thickness uniformity and the like, are improved.
The thickness uniformity test is carried out on the titanium plate prepared in the example 1 and the comparative examples 1-2 with the finished product thickness of 0.39mm, and as can be seen from the table 2, the same plate difference of the titanium plate prepared in the example 1 is 0.011mm, the titanium plate has better thickness uniformity, subsequent correction or finishing procedures are not needed, the correction time is short, and the effect is good. Comparative examples 1 and 2 are insufficient in grain refinement, significant in sheet anisotropy, and low in performance and dimensional stability due to unidirectional rolling of the whole hot rolling process, and comparative example 1 is still insufficient in thickness uniformity though it is subjected to two times of cold rolling and intermediate annealing treatments, and final step annealing treatment. In contrast, comparative example 2, in which the intermediate annealing treatment was not performed in the two cold rolling treatments and the annealing treatment method generally used in the art was finally performed, the annealing treatment was insufficient and the thickness uniformity was significantly lower than those of the previous examples and comparative examples.
According to the invention, the process links are scientifically designed and combined according to the performance and the processing characteristics of the titanium material, and suitable process parameters are obtained through a large number of experiments, so that the limitation of the titanium material processing on equipment is effectively reduced, the simple processing method of the titanium plate special for deep drawing is provided, the performance and the size of the prepared titanium plate are stable, and the titanium plate is beneficial to popularization and application in the fields of medical treatment, environmental protection, aerospace and the like.
The foregoing describes preferred embodiments of the present invention, and is intended to provide a clear and concise description of the spirit and scope of the invention, and not to limit the same, but to include all modifications, substitutions, and alterations falling within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a titanium plate for deep drawing is characterized by comprising the following steps:
the method comprises the following steps: the Brinell hardness HB of the alloy is less than 95 and is 0 A The titanium sponge grade is taken as a raw material, and a titanium ingot is obtained by twice smelting by a vacuum consumable arc smelting method;
step two: forging the titanium ingot in a one-way mode along the axial direction to obtain a titanium plate blank;
step three: hot rolling and cogging, heating the titanium plate blank to 800-850 ℃, and rolling along the direction vertical to the forging direction to obtain a rough rolling blank, wherein the deformation rate is more than 85%; carrying out alkaline acid washing treatment and coping treatment on the rough rolling blank;
step four: hot rolling on second fire, heating the rough rolling blank to 750-800 ℃, rolling along the rolling direction in the third step, wherein the deformation rate is more than 65%, and performing fixed width shearing to obtain a second fire plate blank;
step five: hot rolling with three heats, heating the second hot plate blank to 750-800 ℃, rolling along the direction vertical to the rolling direction of the fourth step, and the deformation rate is more than 35%;
step six: sequentially carrying out a first round of alkali-acid washing treatment, polishing treatment, semi-finished product annealing treatment and a second round of alkali-acid washing treatment on the three fire plate blanks;
step seven: performing cold rolling twice along the rolling direction of the fifth step to obtain a cold-rolled sheet with the thickness of 0.4 +/-0.02;
step eight: and carrying out finished product annealing treatment on the cold-rolled sheet.
2. The method of claim 1, wherein 0 is A The titanium sponge comprises the following components in percentage by mass: less than or equal to 0.03 percent of iron, less than or equal to 0.05 percent of oxygen, less than or equal to 0.01 percent of nitrogen, less than or equal to 0.01 percent of carbon, less than or equal to 0.003 percent of hydrogen, less than or equal to 0.01 percent of silicon, less than or equal to 0.06 percent of chlorine, less than or equal to 0.01 percent of magnesium, less than or equal to 0.01 percent of manganese, less than or equal to 0.01 percent of nickel, less than or equal to 0.01 percent of chromium, less than or equal to 0.02 percent of the sum of other impurities, and the balance of titanium.
3. The production method according to claim 1 or 2, wherein the thickness H x the width B x the length L of the titanium plate blank in the second step is (110 to 135 mm) × (600 to 700 mm) × (1000 to 1200 mm); and in the third step, heating the titanium plate blank to 800-850 ℃, preserving the heat for 120-150min, and rolling to obtain a rough rolling blank with the thickness of 12-15 mm.
4. The preparation method according to claim 3, wherein in the fourth step, the rough rolling blank is heated to 750-800 ℃ and kept for 15-20min for rolling to obtain a two-fire plate blank with the thickness of 3-4 mm; carrying out asynchronous hot rolling on the second hot rolling train by adopting an asynchronous rolling mill set, wherein the asynchronous rolling mill set is provided with at least 1 group of asynchronous rolling mills with different speeds and at least 1 group of asynchronous rolling mills with different diameters; the hot rolling direction is the same as the rolling direction of the step S3.3, and the pressure between the rollers of each rolling mill of the asynchronous rolling mill set is gradually increased along the rolling direction;
upper roll speed V of asynchronous rolling mill 1 : lower roll speed V 2 1.3-1.5, the diameter R of the upper roll of the reducing asynchronous rolling mill 1 : diameter of lower roll R 2 Is 1: (1.1-1.3).
5. The preparation method according to claim 4, wherein in the fifth step, the second fire plate blank is reversed at 90 degrees, heated to 750-800 ℃, and subjected to unidirectional rolling after heat preservation for 10-15min to obtain a third fire plate blank with the thickness of 1.5-2 mm; in the sixth step, the annealing treatment of the semi-finished product comprises:
stacking 3-6 plate blanks;
heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 16-20min.
6. The production method according to claim 4 or 5, wherein the total deformation amount before hot rolling three-fire reversing: the total deformation after hot rolling three-fire reversing is 1-1.15, wherein the total deformation before hot rolling three-fire reversing is (the thickness of a titanium plate blank is H-the thickness of a two-fire plate blank is H) 1 ) H, the total deformation after hot rolling on three heats is (thickness H of the slab on two heats) 1 -finished product thickness H 2 )/H 1 。
7. The preparation method according to claim 6, wherein in the seventh step, the cold rolling is performed once to obtain a cold-rolled blank with the thickness of 0.7-1.0 mm; then rolling to a cold-rolled sheet with the thickness of 0.4 +/-0.02 mm; performing intermediate annealing treatment and alkali-acid washing treatment between two times of cold rolling, wherein the intermediate annealing treatment comprises the following steps:
stacking 3-8 plate blanks;
heating the stacked plate blanks to 680 +/-10 ℃ by adopting an electric furnace, and carrying out annealing treatment for 16-20min.
8. The preparation method according to claim 7, wherein in the eighth step, the single cold-rolled sheet is heated to 680 ± 10 ℃ in-line by using an all-solid-state high-frequency induction heating device, and is annealed for 16-20min.
9. The manufacturing method according to claim 7 or 8, wherein the alkali pickling treatment of the cogged ingot, the triple fire slab and the cold rolled ingot comprises the steps of:
A. alkali washing: soaking the plate blank in alkali melt liquid at 460-520 ℃ and carrying out alkali washing for 5-15min; said alkali melt is composed of 85-95wt% NaOH and 5-15wt% NaNO 3 Forming;
B. primary acid washing: soaking the thin plate blank in a first acid solution at a temperature below 60 DEG CWashing with acid for less than 2min, washing with water and drying; the first acid solution contains: 5-15wt.% of 2 SO 4 And the balance being water;
C. secondary acid washing: soaking the sheet bar in a second acid solution at a temperature below 60 ℃, and pickling for less than 5min; the second acid solution contains: 15-25wt% of HNO 3 1-2% wtHF and the balance water.
10. The manufacturing method according to claim 9, wherein the grinding process for the rough rolled blank and the three-fire plate blank is performed by using a diamond grinding wheel, and comprises the following steps:
s1, coarse grinding: the granularity of the rough grinding wheel is 100-150 meshes, the rotating speed is 1500-2000r/min, the feeding amount is 0.02 mm-0.05 mm each time, and the feeding speed of the diamond grinding wheel is 800 mm/min-1000 mm/min;
s2, fine grinding: the grain size of the fine grinding wheel is 200-300 meshes, the rotating speed is 3500 r/min-4000 r/min, the feeding amount is less than 0.01mm each time, and the feeding speed is 300 mm/min-450 mm/min.
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